CN106243463A - A kind of preparation method of Polymer/nano graphite flake/silicon dioxide composite material - Google Patents
A kind of preparation method of Polymer/nano graphite flake/silicon dioxide composite material Download PDFInfo
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- CN106243463A CN106243463A CN201610763251.4A CN201610763251A CN106243463A CN 106243463 A CN106243463 A CN 106243463A CN 201610763251 A CN201610763251 A CN 201610763251A CN 106243463 A CN106243463 A CN 106243463A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
- B29C45/17—Component parts, details or accessories; Auxiliary operations
- B29C45/76—Measuring, controlling or regulating
- B29C45/77—Measuring, controlling or regulating of velocity or pressure of moulding material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
- B29C45/17—Component parts, details or accessories; Auxiliary operations
- B29C45/76—Measuring, controlling or regulating
- B29C45/78—Measuring, controlling or regulating of temperature
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The present invention relates to polymer composites field, the preparation method of a kind of Polymer/nano graphite flake/silicon dioxide composite material.In the raw material that described composite uses, the particle diameter of thermal expansion graphite is 0.2 ~ 0.6 mm, Nano-meter SiO_22Particle diameter be 9 15nm；This preparation method is by thermal expansion graphite that mass ratio is 3:10 ~ 20:20 ~ 50, Nano-meter SiO_22With polymer by mechanical agitation melt blending, thermal expansion graphite and Nano-meter SiO_22Interaction Force makes thermal expansion graphite peel off in situ and forms nano graphite flakes, prepares Polymer/nano graphite flake/silicon dioxide composite material.The present invention utilizes different dimensions filler to the difference of Shearing Flow response mode in mechanical agitation, set up filler interphase interaction, making thermal expansion graphite peel off in situ and form nano graphite flakes, the original position that can be realized thermal expansion graphite by this kind of configuration control method is peeled off and Nano-meter SiO_22Fine dispersion, make the mechanical property of polymer and hot property be effectively improved simultaneously.
Description
Technical field
The present invention relates to polymer composites field, specifically a kind of Polymer/nano graphite flake/silicon dioxide is combined
The preparation method of material.
Background technology
Polyethylene is as a kind of conventional macromolecular material, due to advantages such as processing characteristics are excellent, cheap, in reality
Life is used widely.But polyethylene itself exists, and mechanical strength is low, non-refractory, the shortcoming such as yielding, in certain journey
Its application in engineering field is limited on degree.At present, existing numerous studies relate to being combined difference filler and polyethylene with
Realize the high performance of polyethylene, Li [Dagang Li, et al.Materials and Design 85 (2015) 54-59] etc.
People is prepared for polyethylene/charcoal powder composite, discusses three kinds of different types of charcoal powders (Masson Pine charcoal, fruit tree Linesless charcoal, bamboo wood
Charcoal) on composite materials property and the impact of electric conductivity, when charcoal powder addition is 70%, the stretching of composite
Intensity carries respectively to 102MPa, 86.8MPa, 72.9MPa, electrical conductivity can reach 3.0 × 10-1S/cm, 3.7 × 10-1S/cm,
3.9×10-1S/cm；Park[Soo-Jin Park,et al.Journal of Industrial and Engineering
Chemistry 21 (2015) 155-157] et al. utilize many walls carbon pipe to improve the capability of electromagnetic shielding of high density polyethylene (HDPE), work as carbon
When pipe content is 18wt%, the capability of electromagnetic shielding of prepared composite can reach 58dB when frequency is 1.4GHZ；Qaiss
[Abou el kacem Qaiss, et al.Mechanics of Materials 98 (2016) 36-43] et al. is by melted
Blend method is prepared for monkey grass/montmorillonite/composite polyethylene material, when the addition of two kinds of fillers is 12.5wt%
Time, the hot strength of composite and Young's modulus can promote 11% and 49%, and the heat stability of material is also with montmorillonite content
Raising and increase.
Graphene nanometer sheet, due to advantages such as its higher Young's modulus, mechanical strength, heat-conductivity conducting performances, becomes polymerization
The important Nano filling [Zhixiong Huang, et al.Composites:Part A87 (2016) 10-22] that thing is modified.Mesh
The front research utilizing graphene nanometer sheet to prepare high-performance polymer nano composite material is the most much reported.Taheri et al.
[F.Taheri, et al.Materials and Design 66 (2015) 142-149] uses modified graphene nanometer sheet to fill
It is prepared for epoxy resin/graphite alkene nano composite material, when modified graphene nanometer sheet addition is 0.5%, compound
The stretch modulus of material and fracture toughness have been respectively increased 15% and 82% than when adding unmodified Graphene.Yu et al.
The method that [Jaesang Yu, et al.Composites:Part A69 (2015) 219-225] passes through to mold is by graphene nano
Sheet is blended with mutual-phenenyl two acid bromide two alcohol ester and is prepared for composite, and is studied its heat conductivity, and research discovery adds
The graphene nanometer sheet adding 20wt% can make the heat conductivity of composite reach 1.98W/mK.But, Graphene price is higher,
And easily reunite in polymeric matrix, therefore utilize Graphene to be modified polymer still suffering from being stranded in actual production
Difficult.
Thermal expansion graphite is obtained through high-temperature process by expansible graphite.Expansible graphite intercalator when being heated decomposes generation
A large amount of expansiveness gases, promote graphite layers to open, make interlayer generation physical expansion, are formed internal thin by a large amount of nano-graphites
" graphite worm " structure of sheet composition.Under the outer field actions such as ultrasonic, shearing, the loosest inside thermal expansion graphite pile up sheet
Rotating fields can be partially stripped, and is formed by several nano graphite flakes formed to tens monolithic layer graphite.
Therefore, with low cost thermal expansion graphite as filler, made by introducing shear action during composite processing
Expanded graphite is peeled off in situ and is generated nano graphite flakes, can realize the effectively dispersion of nano graphite flakes and to polymer high performance
Modified purpose.Preparing high-performance polyethylene nano composite material by above method, its operational approach is simple, with low cost,
And it is easily achieved large-scale production, significant to the range of application widening polyethylene.
Summary of the invention
The present invention has high performance composite to prepare, it is provided that a kind of Polymer/nano graphite flake/titanium dioxide
The preparation method of silicon composite.
The present invention is achieved by the following technical solutions: a kind of Polymer/nano graphite flake/silicon dioxide composite material
Preparation method, in the raw material that described composite uses, the particle diameter of thermal expansion graphite is 0.2～0.6mm, Nano-meter SiO_22Grain
Footpath is 9-15nm；This preparation method is by thermal expansion graphite that mass ratio is 3:10～20:20～50, Nano-meter SiO_22With polymer
By mechanical agitation melt blending, thermal expansion graphite and Nano-meter SiO_22Interaction Force makes thermal expansion graphite peel off shape in situ
Become nano graphite flakes, prepare Polymer/nano graphite flake/silicon dioxide composite material (masterbatch).
It is 10～20:3 that composite of the present invention (masterbatch) introduces with thermal expansion graphite quality ratio in preparation process
Nano-meter SiO_22, utilize different dimensions filler (thermal expansion graphite, Nano-meter SiO_22) to Shearing Flow response mode in mechanical agitation
Difference, sets up filler interphase interaction, makes thermal expansion graphite peel off in situ and forms nano graphite flakes, makes Nano-meter SiO_2 simultaneously2Point
Dissipate property to improve；The original position that can be realized thermal expansion graphite by this kind of configuration control method is peeled off and Nano-meter SiO_22Good point
Dissipate, make the mechanical property of polymer and hot property be effectively improved simultaneously.Composite of the present invention (masterbatch) relative to
Directly use nano graphite flakes, Nano-meter SiO_22With polymer be blended composite, have with low cost, easy and simple to handle, be prone to
Realize the advantage such as large-scale production and nanoparticle favorable dispersibility.
Test shows, only in the range of the particle diameter and mass ratio of raw material of the present invention, thermal expansion graphite just can be former
Position is peeled off and is formed nano graphite flakes, simultaneously Nano-meter SiO_22Aggregate dispersibility improves；According to other particle diameters or mass ratio, then difficult
To realize being effectively peeled off and Nano-meter SiO_2 of graphite flake layer2The fine dispersion of particle.
In order to dilute masterbatch further, reducing filer content, the present invention enters on the basis of above-mentioned composite (masterbatch)
One step adds Nano-meter SiO_22With polymer by after melt blending, pelletize, vacuum drying, it is thus achieved that polymer content be 88.5～
89.5wt%, nano graphite flakes content is 0.5～1.5wt% and Nano-meter SiO_22Content is the high performance composite of 10wt%
Material.
When being embodied as, it is real in torque rheometer for preparing the mechanical agitation melt blending used by composite (masterbatch)
Execute, add Nano-meter SiO_2 further2Implement in double screw extruder with the melt blending after polymer.
Further, described polymer is polyethylene.Certainly, when implementing technical scheme of the present invention, it is not limited to
Polythene material, also can use other thermoplastic macromolecule materials when implementing.
When the polymer used is polyethylene, in torque rheometer, the mechanical agitation melt blending of material is 135
～140 DEG C of realizations.In double screw extruder, the melt blending of material is 165～190 DEG C of realizations.
Preferably, the temperature that pelletize final vacuum is dried is 40～60 DEG C, and drying time is 12～24h.
In order to the performance of high-performance composite materials is measured, after pelletize, vacuum drying by injection machine 170～
200 DEG C, injection mo(u)lding under pressure 35-40MPa.
Accompanying drawing explanation
Fig. 1 is PE/SiO2And PE/GNPs/SiO2The stereoscan photograph of composite.As seen from the figure, PE/SiO2Compound
SiO in material2Dispersibility poor, mean diameter is about 450nm, and thermal expansion graphite add after PE/GNPs/SiO2Composite wood
SiO in material2Size substantially reduce, its mean diameter is reduced to about 300nm, illustrates that this preparation method can effectively realize
SiO2Fine dispersion.
Fig. 2 is PE/GNPs/SiO2The transmission electron microscope photo of composite.As seen from the figure, nano graphite flakes is dispersed in
In PE matrix, particle diameter is about 40nm, it was demonstrated that this preparation method can make thermal expansion graphite peel off in situ and generate nano-graphite
Sheet.
Fig. 3, Fig. 4, Fig. 5 are respectively the stretching of high-performance composite materials, bending, heat resistance curve chart.From figure permissible
Find out, compared with pure polyethylene, PE/GNPs/nano-SiO2The stretching of composite, bending, heat resistance all obtain different journey
The raising of degree.
Detailed description of the invention
Embodiment one:
The preparation method of a kind of high-performance composite materials comprises the steps:
(1) being taken out immediately after thermal expansion 40s in the Muffle furnace of 900 DEG C by expansible graphite, room temperature cools down；
(2) being scattered in dehydrated alcohol by the product obtained by step (1), process 1h in Ultrasonic Cell Disruptor, room temperature is waved
Send out dehydrated alcohol, place into after ethanol volatilization completely in 80 DEG C of vacuum drying ovens and be dried 24h；
(3) by the thermal expansion graphite that particle diameter is 0.2～0.6mm obtained by step (2), it is the nanometer of 9-15nm with particle diameter
SiO2In torque rheometer, composite is prepared with polyethylene 3:10:30 in mass ratio, at 190 DEG C, the condition of rotating speed 40rpm
Lower use parallel dual-screw extruding machine carries out masterbatch dilution so that nano graphite flakes and nano silicon and polyethylene in system
Percent content is respectively 0.5wt%, 10wt%, 89.5wt%, is dried 12h, by note after pelletize in 50 DEG C of vacuum drying ovens
Molding machine is at 200 DEG C, and under pressure 40MPa, injection mo(u)lding prepares high performance PE/GNPs/SiO2Composite batten.
Embodiment two:
The preparation method of a kind of high-performance composite materials comprises the steps:
(1) being taken out immediately after thermal expansion 40s in the Muffle furnace of 900 DEG C by expansible graphite, room temperature cools down；
(2) being scattered in dehydrated alcohol by the product obtained by step (1), process 1h in Ultrasonic Cell Disruptor, room temperature is waved
Send out dehydrated alcohol, place into after ethanol volatilization completely in 80 DEG C of vacuum drying ovens and be dried 24h；
(3) by the thermal expansion graphite that particle diameter is 0.2～0.6mm obtained by step (2), it is the nanometer of 9-15nm with particle diameter
SiO2In torque rheometer, composite is prepared with polyethylene 3:10:30 in mass ratio, at 190 DEG C, the condition of rotating speed 40rpm
Lower use parallel dual-screw extruding machine carries out masterbatch dilution so that nano graphite flakes and nano silicon and polyethylene in system
Percent content is respectively 1wt%, 10wt%, 89wt%, is dried 12h, passes through injection machine after pelletize in 50 DEG C of vacuum drying ovens
At 200 DEG C, under pressure 40MPa, injection mo(u)lding prepares high performance PE/GNPs/SiO2Composite batten.
Embodiment three:
The preparation method of a kind of high-performance composite materials comprises the steps:
(1) being taken out immediately after thermal expansion 40s in the Muffle furnace of 900 DEG C by expansible graphite, room temperature cools down；
(2) being scattered in dehydrated alcohol by the product obtained by step (1), process 1h in Ultrasonic Cell Disruptor, room temperature is waved
Send out dehydrated alcohol, place into after ethanol volatilization completely in 80 DEG C of vacuum drying ovens and be dried 24h；
(3) by the thermal expansion graphite that particle diameter is 0.2～0.6mm obtained by step (2), it is the nanometer of 9-15nm with particle diameter
SiO2In torque rheometer, composite is prepared with polyethylene 3:10:30 in mass ratio, at 190 DEG C, the condition of rotating speed 40rpm
Lower use parallel dual-screw extruding machine carries out masterbatch dilution so that nano graphite flakes and nano silicon and polyethylene in system
Percent content is respectively 1.5wt%, 10wt%, 88.5wt%, is dried 12h, by note after pelletize in 50 DEG C of vacuum drying ovens
Molding machine is at 200 DEG C, and under pressure 40MPa, injection mo(u)lding prepares high performance PE/GNPs/SiO2Composite batten.
Embodiment four:
The preparation method of a kind of high-performance composite materials comprises the steps:
(1) being taken out immediately after thermal expansion 40s in the Muffle furnace of 900 DEG C by expansible graphite, room temperature cools down；
(2) being scattered in dehydrated alcohol by the product obtained by step (1), process 1h in Ultrasonic Cell Disruptor, room temperature is waved
Send out dehydrated alcohol, place into after ethanol volatilization completely in 80 DEG C of vacuum drying ovens and be dried 24h；
(3) by the thermal expansion graphite that particle diameter is 0.2～0.6mm obtained by step (2), it is the nanometer of 9-15nm with particle diameter
SiO2In torque rheometer, composite is prepared with polyethylene 3:15:20 in mass ratio, at 190 DEG C, the condition of rotating speed 40rpm
Lower use parallel dual-screw extruding machine carries out masterbatch dilution so that nano graphite flakes and nano silicon and polyethylene in system
Percent content is respectively 1.5wt%, 10wt%, 88.5wt%, is dried 12h, by note after pelletize in 50 DEG C of vacuum drying ovens
Molding machine is at 200 DEG C, and under pressure 40MPa, injection mo(u)lding prepares high performance PE/GNPs/SiO2Composite batten.
Embodiment five:
The preparation method of a kind of high-performance composite materials comprises the steps:
(1) being taken out immediately after thermal expansion 40s in the Muffle furnace of 900 DEG C by expansible graphite, room temperature cools down；
(2) being scattered in dehydrated alcohol by the product obtained by step (1), process 1h in Ultrasonic Cell Disruptor, room temperature is waved
Send out dehydrated alcohol, place into after ethanol volatilization completely in 80 DEG C of vacuum drying ovens and be dried 24h；
(3) by the thermal expansion graphite that particle diameter is 0.2～0.6mm obtained by step (2), it is the nanometer of 9-15nm with particle diameter
SiO2In torque rheometer, composite is prepared with polyethylene 3:20:50 in mass ratio, at 190 DEG C, the condition of rotating speed 40rpm
Lower use parallel dual-screw extruding machine carries out masterbatch dilution so that nano graphite flakes and nano silicon and polyethylene in system
Percent content is respectively 1.0wt%, 10wt%, 89wt%, is dried 12h, by injection after pelletize in 50 DEG C of vacuum drying ovens
Machine is at 200 DEG C, and under pressure 40MPa, injection mo(u)lding prepares high performance PE/GNPs/SiO2Composite batten.
Following table is that embodiment one is to the composite stretching obtained by embodiment three, heat resistance contrast table
Claims (7)
1. the preparation method of Polymer/nano graphite flake/silicon dioxide composite material, it is characterised in that described composite wood
In the raw material that material uses, the particle diameter of thermal expansion graphite is 0.2 ~ 0.6 mm, Nano-meter SiO_22Particle diameter be 9-15nm；This preparation method
It is by thermal expansion graphite that mass ratio is 3:10 ~ 20:20 ~ 50, Nano-meter SiO_22With polymer by mechanical agitation melt blending, heat
Expanded graphite and Nano-meter SiO_22Interaction Force makes thermal expansion graphite peel off in situ and forms nano graphite flakes, prepares polymerization
Thing/nano graphite flakes/silicon dioxide composite material.
The preparation method of a kind of Polymer/nano graphite flake/silicon dioxide composite material the most according to claim 1, its
Being characterised by, described Polymer/nano graphite flake/silicon dioxide composite material adds Nano-meter SiO_2 further2Pass through with polymer
After melt blending, pelletize, vacuum drying, it is thus achieved that polymer content is 88.5 ~ 89.5 wt%, nano graphite flakes content is 0.5 ~
1.5 wt% and Nano-meter SiO_22Content is the high-performance composite materials of 10 wt%.
The preparation method of Polymer/nano graphite flake/silicon dioxide composite material the most according to claim 1 and 2, it is special
Levying and be, described mechanical agitation melt blending is implemented in torque rheometer, adds Nano-meter SiO_2 further2And polymer
After melt blending implement in double screw extruder.
The preparation method of Polymer/nano graphite flake/silicon dioxide composite material the most according to claim 3, its feature
Being, described polymer is selected from thermoplastic macromolecule material, preferably polyethylene.
The preparation method of Polymer/nano graphite flake/silicon dioxide composite material the most according to claim 4, its feature
Being, in torque rheometer, the mechanical agitation melt blending of material is 135 ~ 140 DEG C of realizations.
The preparation method of Polymer/nano graphite flake/silicon dioxide composite material the most according to claim 5, its feature
Being, in double screw extruder, the melt blending of material is 165 ~ 190 DEG C of realizations.
The preparation method of Polymer/nano graphite flake/silicon dioxide composite material the most according to claim 6, its feature
Being, the temperature that pelletize final vacuum is dried is 40 ~ 60 DEG C, and drying time is 12 ~ 24h.
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Cited By (3)
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| CN107815114A (en) * | 2017-10-11 | 2018-03-20 | 上海阿莱德实业股份有限公司 | A kind of flexible compound graphite-based material for possessing high thermal conductivity energy and preparation method thereof |
| CN111320868A (en) * | 2018-12-17 | 2020-06-23 | 杜邦聚合物有限公司 | Polymer composition with high dielectric constant and low dielectric loss |
| CN112142041A (en) * | 2020-09-30 | 2020-12-29 | 南通大学 | Quartz fiber solid waste SiO2Transformation and utilization method of |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107815114A (en) * | 2017-10-11 | 2018-03-20 | 上海阿莱德实业股份有限公司 | A kind of flexible compound graphite-based material for possessing high thermal conductivity energy and preparation method thereof |
| CN111320868A (en) * | 2018-12-17 | 2020-06-23 | 杜邦聚合物有限公司 | Polymer composition with high dielectric constant and low dielectric loss |
| CN111320868B (en) * | 2018-12-17 | 2023-02-28 | 杜邦聚合物有限公司 | Polymer composition with high dielectric constant and low dielectric loss |
| CN112142041A (en) * | 2020-09-30 | 2020-12-29 | 南通大学 | Quartz fiber solid waste SiO2Transformation and utilization method of |
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| Publication number | Publication date |
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| CN106243463B (en) | 2018-10-23 |
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